CN106366203B - A kind of preparation method of Cardia Salt carboxymethyl cellulose lithium - Google Patents
A kind of preparation method of Cardia Salt carboxymethyl cellulose lithium Download PDFInfo
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- CN106366203B CN106366203B CN201610792899.4A CN201610792899A CN106366203B CN 106366203 B CN106366203 B CN 106366203B CN 201610792899 A CN201610792899 A CN 201610792899A CN 106366203 B CN106366203 B CN 106366203B
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- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
- C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
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Abstract
The invention belongs to natural polymer field of chemical modification, and in particular to a kind of preparation method of Cardia Salt carboxymethyl cellulose lithium.Technical problem to be solved by the invention is to provide a kind of preparation methods of carboxymethyl cellulose lithium, comprising the following steps: A, acidification: in organic solvent by acid solution dispersion, sodium carboxymethylcellulose is added, obtains mixed solution 1；It is reacted at 50~75 DEG C, takes off liquid after reaction, obtain crude product carboxymethyl cellulose acid；It washs and takes off liquid；B, lithiumation: in organic solvent by the dispersion of carboxymethyl cellulose acid, LiOH aqueous solution is added, obtains mixed solution 2；It is reacted at 10~40 DEG C, being neutralized to pH after reaction is 7~8, takes off liquid, obtains crude product carboxymethyl cellulose lithium；Washing, de- liquid, drying, crushing obtain finished product carboxymethyl cellulose lithium.The carboxymethyl cellulose lithium of Cardia Salt can be prepared in the method for the present invention.
Description
Technical field
The invention belongs to natural polymer field of chemical modification, and in particular to a kind of system of Cardia Salt carboxymethyl cellulose lithium
Preparation Method.
Background technique
CN101942028A describes a kind of preparation process of food-grade potassium carboxymethylcellulose, and method is first toward food
The sulfuric acid of addition 10%~40% is acidified in grade sodium carboxymethylcellulose, reacts in certain temperature and under the time to obtain carboxylic
Methylcellulose acid crude obtains carboxymethyl cellulose acid sterling by washing, dehydration, drying and crushing, adds K2CO3/
(NH4)2CO3Equal solid bases are neutralized, and potassium carboxymethylcellulose is obtained.
CN102206286A describes a kind of preparation process of carboxymethyl cellulose lithium, and method is first toward in slurry processes system
The hydrochloric acid of addition 15%~25% is acidified in the sodium carboxymethylcellulose obtained, and certain time is reacted at 20 DEG C~50 DEG C and is obtained
To carboxymethyl cellulose crude product, obtained by organic solvent washing, dehydration, drying and crushing that volumetric concentration is 80%~95%
Carboxymethyl cellulose acid sterling, adds LiOH.H2O aqueous solution reacted at 40 DEG C~60 DEG C after a certain period of time with glacial acetic acid into
Row neutralizes, and then obtains carboxymethyl cellulose lithium with certain density organic solvent washing, de- liquid, drying and crushing.This method
The sodium carboxymethylcellulose for being selected to slurry processes preparation is raw material, and degree of substitution is higher, and acidization is inorganic non-oxygen using low concentration
The property changed acid is acidified, then is washed with high levels of organic solvents, which will lead to original sodium carboxymethylcellulose acidification
Not exclusively, unreacted sodium carboxymethylcellulose remains in system, at the same its in alkalinization by reaction system temperature
Degree, which is turned up, is unfavorable for carboxymethyl cellulose acid and lye progress neutralization reaction, and eventually leads to the pure of practical carboxymethyl cellulose lithium
It spends low.
Summary of the invention
Goal of the invention of the invention is to provide the carboxymethyl cellulose lithium of sodium salt content < 0.1% a kind of.The carboxymethyl
Cellulose lithium is applied to that the internal resistance of lithium battery can be reduced when lithium battery binder, the charge and discharge number for increasing lithium battery, extends
The service life of lithium battery.
The technical solution of present invention solution above-mentioned technical problem, comprising the following steps:
A, it is acidified:
A, in organic solvent by acid solution dispersion, sodium carboxymethylcellulose is added, obtains mixed solution 1；Wherein, it mixes
The mass concentration of organic solvent is 50~90% in 1 system of solution；The acid solution is at least one of sulfuric acid or nitric acid；
B, mixed solution 1 reacts at 50~75 DEG C, removes liquid after reaction, obtains crude product carboxymethyl cellulose
Acid；
C, crude product carboxymethyl cellulose acid is washed with solvent, and removes liquid；The solvent is mass concentration≤50%
Organic solvent or water；
B, lithiumation:
D, step c is washed and removes the dispersion of the carboxymethyl cellulose acid after liquid in organic solvent, hydroxide is added
Lithium aqueous solution obtains mixed solution 2；
E, mixed solution 2 reacts at 10~40 DEG C, and being neutralized to pH after reaction is 7~8, removes liquid, obtains thick
Product carboxymethyl cellulose lithium；
F, with organic solvent washing crude product carboxymethyl cellulose lithium, removing liquid, drying, crushing obtain finished product carboxymethyl fibre
Tie up plain lithium.
Preferably, in above method step a, the mass concentration of the acid solution is 10~65%.
Preferably, in above method step a, the mass ratio of the acid solution and sodium carboxymethylcellulose is 1~5 ︰ 3；Bath
It is 1 ︰ 4~9 than control；The bath raio is the mass ratio of sodium carboxymethylcellulose and system liquid summation.
Preferably, in above method step b, the reaction time is 1~4h.
Preferably, in above method step d, in 2 system of mixed solution the mass concentration of organic solvent be 50~
90%.
Preferably, in above method step d, the lithium hydroxide aqueous solution mass concentration is 8~13%.
Preferably, in above method step d, the mass ratio of the lithium hydroxide aqueous solution and carboxymethyl cellulose acid is 6
~12 ︰ 7；Bath raio control is 1 ︰ 5~10；The bath raio is the mass ratio of carboxymethyl cellulose acid and system liquid summation.
Preferably, in above method step e, the reaction time is 1~4h.
Preferably, in above method step e, described neutralize is neutralized using acetic acid.
Preferably, in above method step f, the organic solvent mass concentration is 75~95%.
Preferably, in the above method, the organic solvent is at least one in ethyl alcohol, isopropanol, the tert-butyl alcohol or acetone
Kind.
The method of the present invention is by adjusting optimizing the concentration of organic solvent in acid system, sour type, souring temperature, acidification
The technological parameters such as washing conditions afterwards have finally prepared sodium salt in 0.1% carboxymethyl cellulose lithium below.
Specific embodiment
A kind of preparation method of the carboxymethyl cellulose lithium of Cardia Salt, comprising the following steps:
A, it is acidified:
A, in organic solvent by acid solution dispersion, sodium carboxymethylcellulose is added, obtains mixed solution 1；Wherein, it mixes
The mass concentration of organic solvent is 50~90% in 1 system of solution；The acid solution is at least one of sulfuric acid or nitric acid；
The organic solvent is at least one of ethyl alcohol, isopropanol, the tert-butyl alcohol or acetone；
B, mixed solution 1 reacts at 50~75 DEG C, carries out centrifugation removing liquid after reacting 1~4h, obtains crude product carboxylic first
Base cellulosic acid；
C, crude product carboxymethyl cellulose acid is washed with solvent, and is centrifuged removing liquid；The solvent be mass concentration≤
50% organic solvent or water；The organic solvent is at least one of ethyl alcohol, isopropanol, the tert-butyl alcohol or acetone；
B, lithiumation:
D, step c is washed and removes the dispersion of the carboxymethyl cellulose acid after liquid in organic solvent, hydroxide is added
Lithium aqueous solution obtains mixed solution 2；The organic solvent is at least one of ethyl alcohol, isopropanol, the tert-butyl alcohol or acetone；
E, mixed solution 2 reacts 1~4h at 10~40 DEG C, uses in acetic acid and system to pH is 7~8, centrifugation removes
Liquid obtains crude product carboxymethyl cellulose lithium；
F, with organic solvent washing crude product carboxymethyl cellulose lithium, centrifugation removing liquid, drying, crushing obtain finished product carboxylic first
Base cellulose lithium；The organic solvent is at least one of ethyl alcohol, isopropanol, the tert-butyl alcohol or acetone.
Preferably, in above method step a, the mass concentration of the acid solution is 10~65%.
Preferably, in above method step a, the mass ratio of the acid solution and sodium carboxymethylcellulose is 1~5 ︰ 3, bath
It is 1 ︰ 4~9 than control；The bath raio is the mass ratio of sodium carboxymethylcellulose and system liquid summation.
Preferably, in above method step d, in 2 system of mixed solution the mass concentration of organic solvent be 50~
90%.
Preferably, in above method step d, the lithium hydroxide aqueous solution mass concentration is 8~13%.
Preferably, in above method step d, the mass ratio of the lithium hydroxide aqueous solution and carboxymethyl cellulose acid is 6
~12 ︰ 7；Bath raio control is 1 ︰ 5~10；The bath raio is the mass ratio of carboxymethyl cellulose acid and system liquid summation.By
The carboxymethyl cellulose acid of step c centrifugation removing liquid is wet carboxymethyl cellulose acid, also contains a large amount of solvent, so,
The additive amount for the carboxymethyl cellulose acid that step d is related to indicates the carboxymethyl cellulose acid of dry material.
Preferably, in above method step f, the organic solvent mass concentration is 75~95%.
For the defect of existing carboxymethyl cellulose lithium, the present inventor carries out the preparation method of carboxymethyl cellulose lithium
It researchs and analyses, technical solution of the present invention has finally been determined by a large number of experiments.The method of the present invention passes through reasonably control acidification
In system the concentration of organic solvent with ensure be acidified uniformity, because if concentration cross low reaction will be incomplete, excessive concentration
It will lead to that material viscosity reduction is serious, directly affect the use cost of user；Reaction temperature is changed in acidization simultaneously, makes body
Molecular motion is more active in system, reacts more evenly；Secondly carboxymethyl cellulose lithium solution is further improved with oxidizing acid
Transparency, acidification reaction are more thorough；With the insoluble CMC-H of solvent washing water of high water content, it is more advantageous to the removing of sodium salt；
Lithiumation is carried out with lithium hydroxide aqueous solution, is more advantageous to the generation of CMC-Li；Lithiation temperature is changed simultaneously, acid is more advantageous to
Alkali neutralization exothermic reaction is carried out to positive reaction direction, and lithiation is more thorough.The each technological parameter of the method for the present invention complements each other,
Sodium salt content finally has been prepared in 0.1% carboxymethyl cellulose lithium below.
Embodiment 1
(1) acidization of sodium carboxymethylcellulose:
To mediate the physical and chemical index of the sodium carboxymethylcellulose of method preparation are as follows: degree of substitution DS=0.92,1% solution viscosity
1392cp, purity 98.5% are used as raw material；It disperses the sulfuric acid solution 250g that mass concentration is 25% in aqueous isopropanol, adds
Enter 150g sodium carboxymethylcellulose, control system isopropanol organic solvent concentration is 68%, and bath raio is 1 ︰ 9, is reacted at 50 DEG C
4h washs obtained carboxymethyl cellulose acid 2 times with concentration after centrifugation for 40% aqueous isopropanol, and centrifugation is stand-by；
(2) the lithiumation process of carboxymethyl cellulose acid:
130g CMC-H (is given money as a gift), 95% isopropanol water system is scattered in, the LiOH that 150g mass concentration is 8% is added
Aqueous solution, control system isopropyl alcohol concentration are 76%, and bath raio is 1 ︰ 10, uses acetic acid after above-mentioned mixed liquor is reacted 4h at 20 DEG C
It is neutralized to PH=7.5；Centrifugal dewatering is washed 1 time, 80% ethanol washing 1 time with the aqueous isopropanol of concentration 75%, centrifugation,
It dries, crush to obtain carboxymethyl cellulose lithium.
CMC-Li:DS=0.90 obtained by the present embodiment, 1% solution viscosity 1255cp, aqueous solution light transmittance 98.8% are pure
Spend 99.2%, Na salt=0.092%wt, lithiumation rate=97.8%.
Embodiment 2
(1) acidization of sodium carboxymethylcellulose:
To mediate the physical and chemical index of the sodium carboxymethylcellulose of method preparation are as follows: degree of substitution DS=0.89,1% solution viscosity
40cp, purity 98% are used as raw material.It disperses the sulfuric acid solution 180g that mass concentration is 40% in ethanol water, is added
150g sodium carboxymethylcellulose, control system concentration of alcohol are 65%, and bath raio is 1 ︰ 7；2.5h is reacted at 55 DEG C, it will after centrifugation
Obtained carboxymethyl cellulose acid is that 38% ethanol solution washs 3 times with concentration, and centrifugation is stand-by；
(2) the lithiumation process of carboxymethyl cellulose acid: 130g CMC-H (being given money as a gift), 95% ethanolic aqueous system is scattered in,
The LiOH aqueous solution that 130g mass concentration is 10% is added, control system concentration of alcohol is 80%, and bath raio is 1 ︰ 10, will be above-mentioned mixed
It closes liquid and is reacted at 25 DEG C and be neutralized to PH=7.2 with acetic acid after 3h；Centrifugal dewatering is washed 2 times with the ethanol solution of concentration 75%,
80% ethanol washing 2 times is centrifuged, dries, crushing and to obtain carboxymethyl cellulose lithium.
CMC-Li:DS=0.81 obtained by the present embodiment, 1% solution viscosity 39cp, aqueous solution light transmittance 98.5%, purity
98%, Na salt=0.088%wt, lithiumation rate=91%.
Embodiment 3
(1) acidization of sodium carboxymethylcellulose:
To mediate the physical and chemical index of the sodium carboxymethylcellulose of method preparation are as follows: degree of substitution DS=0.90,1% solution viscosity
988cp, purity 98.5% are used as raw material.The sulfuric acid and nitric acid mixed solution for being 45% by mass concentration (mass ratio is 1 ︰ 1)
135g is scattered in aqueous acetone solution, and 150g sodium carboxymethylcellulose is added, and control system concentration of alcohol is 78%, and bath raio is 1 ︰
10；2h is reacted at 55 DEG C, softens obtained carboxymethyl cellulose acid water washing 3 times after centrifugation, and centrifugation is stand-by；
(2) the lithiumation process of carboxymethyl cellulose acid:
130g CMC-H (is given money as a gift), is scattered in pure C ketone solvent, the LiOH water that 110g mass concentration is 12% is added
Solution, control system concentration of alcohol are 78%, and bath raio is 1 ︰ 7, above-mentioned mixed liquor react at 18 DEG C after 4h in acetic acid with
To PH=7.0；Centrifugal dewatering is washed 3 times, 80% ethanol washing 2 times with the ethanol solution of concentration 75%, centrifugation, drying, powder
It is broken to obtain carboxymethyl cellulose lithium.
CMC-Li:DS=0.88 obtained by the present embodiment, 1% solution viscosity 760cp, aqueous solution light transmittance 98.2% are pure
Spend 99.4%, Na salt=0.071%wt, lithiumation rate=97.7%.
Embodiment 4
(1) acidization of sodium carboxymethylcellulose:
To mediate the physical and chemical index of the sodium carboxymethylcellulose of method preparation are as follows: degree of substitution DS=0.93,1% solution viscosity
4600cp, purity 98% are used as raw material.Disperse the nitric acid solution 240g that mass concentration is 38% in 95% ethanol water
In, 150g sodium carboxymethylcellulose is added, control system concentration of alcohol is 75%, and bath raio is 1 ︰ 9；2h is reacted at 65 DEG C, from
Obtained carboxymethyl cellulose acid is washed 2 times with concentration for 35% ethanol solution after the heart, centrifugation is stand-by；
(2) the lithiumation process of carboxymethyl cellulose acid:
130g CMC-H (is given money as a gift), 95% ethanolic aqueous system is scattered in, the LiOH water that 140g mass concentration is 9% is added
Solution, control system concentration of alcohol are 78%, and bath raio is 1 ︰ 10, above-mentioned mixed liquor react at 40 DEG C after 2h in acetic acid with
To PH=7.3；Centrifugal dewatering is washed 2 times, 80% ethanol washing 2 times with the ethanol solution of concentration 75%, centrifugation, drying, powder
It is broken to obtain carboxymethyl cellulose lithium.
CMC-Li:DS=0.88 obtained by the present embodiment, 1% solution viscosity 4333cp, aqueous solution light transmittance 98.5% are pure
Spend 98.5%, Na salt=0.084%wt, lithiumation rate=94.6%.
Embodiment 5
(1) acidization of sodium carboxymethylcellulose:
To mediate the physical and chemical index of the sodium carboxymethylcellulose of method preparation are as follows: degree of substitution DS=0.85,1% solution viscosity
6339cp, purity 98.8% are used as raw material.It disperses the nitric acid solution 100g that mass concentration is 66% in aqueous isopropanol, adds
Enter 150g sodium carboxymethylcellulose, control system isopropyl alcohol concentration is 72%, and bath raio is 1 ︰ 7；3h is reacted at 60 DEG C, after centrifugation
Obtained carboxymethyl cellulose acid is washed 3 times with concentration for 40% aqueous isopropanol, centrifugation is stand-by；
(2) the lithiumation process of carboxymethyl cellulose acid:
130g CMC-H (is given money as a gift), 95% isopropanol water system is scattered in, the LiOH that 160g mass concentration is 9% is added
Aqueous solution, control system isopropyl alcohol concentration are 75%, and bath raio is 1 ︰ 9, uses acetic acid after above-mentioned mixed liquor is reacted 3h at 36 DEG C
It is neutralized to PH=7.8；It is washed 1 time with the ethanol solution of concentration 70%, 75% ethanol washing 2 times is centrifuged, dries, crushes
Carboxymethyl cellulose lithium.
CMC-Li:DS=0.83 obtained by the present embodiment, 1% solution viscosity 6130cp, aqueous solution light transmittance 98.5% are pure
Spend 99.0%, Na salt=0.081%wt, lithiumation rate=97.6%.
Embodiment 6
(1) acidization of sodium carboxymethylcellulose:
To mediate the physical and chemical index of the sodium carboxymethylcellulose of method preparation are as follows: degree of substitution DS=0.89,1% solution viscosity
6339cp, purity 98.8% are used as raw material.The nitric acid and sulfuric acid mixing (mass ratio is 1 ︰ 1) solution for being 40% by mass concentration
100g is scattered in aqueous isopropanol, and 150g sodium carboxymethylcellulose is added, and control system isopropyl alcohol concentration is 72%, and bath raio is
1 ︰ 7；1h is reacted at 50 DEG C, washs obtained carboxymethyl cellulose acid 3 times for 40% ethanol solution with concentration after centrifugation, from
The heart is stand-by；
(2) the lithiumation process of carboxymethyl cellulose acid:
130g CMC-H (is given money as a gift), 95% ethanolic aqueous system is scattered in, the LiOH that 160g mass concentration is 10% is added
Aqueous solution, control system isopropyl alcohol concentration are 82%, and bath raio is 1 ︰ 9, uses vinegar after above-mentioned mixed liquor is reacted 2.5h at 33 DEG C
Acid is neutralized to PH=7.8；It is washed 3 times with the ethanol solution of concentration 80%, is centrifuged, dries, crushing and to obtain carboxymethyl cellulose lithium.
CMC-Li:DS=0.86 obtained by the present embodiment, 1% solution viscosity 3561cp, aqueous solution light transmittance 98.1% are pure
Spend 99.0%, Na salt=0.058%wt, lithiumation rate=96.6%.
Claims (9)
1. a kind of preparation method of Cardia Salt carboxymethyl cellulose lithium, it is characterised in that: the following steps are included:
A, it is acidified:
A, acid solution is dispersed in organic solvent solution, sodium carboxymethylcellulose is added, obtains mixed solution 1；Wherein, it mixes
The mass concentration of organic solvent is 50~90% in 1 system of solution；The acid solution is at least one of sulfuric acid or nitric acid；
B, mixed solution 1 reacts at 50~75 DEG C, removes liquid after reaction, obtains crude product carboxymethyl cellulose acid；
C, crude product carboxymethyl cellulose acid is washed with solvent, and removes liquid；The solvent is the organic of mass concentration≤50%
Solvent solution or water；
B, lithiumation:
D, step c is washed and removes the carboxymethyl cellulose acid after liquid and be dispersed in organic solvent solution, hydroxide is added
Lithium aqueous solution obtains mixed solution 2；
E, mixed solution 2 reacts at 10~40 DEG C, and being neutralized to pH after reaction is 7~8, removes liquid, obtains crude product carboxylic
Methylcellulose lithium；
F, crude product carboxymethyl cellulose lithium is washed with organic solvent solution, removing liquid, drying, crushing obtain finished product carboxymethyl fibre
Tie up plain lithium.
2. according to the method described in claim 1, it is characterized by: in step a, the mass concentration of the acid solution is 10~
65%.
3. according to the method described in claim 1, it is characterized by: in step a, the acid solution and sodium carboxymethylcellulose
Mass ratio is 1~5 ︰ 3；Bath raio control is 1 ︰ 4~9；The bath raio is the matter of sodium carboxymethylcellulose and system liquid summation
Amount ratio.
4. according to the method described in claim 1, it is characterized by: in step d, organic solvent in 2 system of mixed solution
Mass concentration be 50~90%.
5. according to the method described in claim 1, it is characterized by: in step d, the lithium hydroxide aqueous solution mass concentration is
8~13%.
6. according to the method described in claim 1, it is characterized by: the lithium hydroxide aqueous solution and carboxymethyl are fine in step d
The mass ratio of dimension element acid is 6~12 ︰ 7；Bath raio control is 1 ︰ 5~10；The bath raio is carboxymethyl cellulose acid and system liquid
The mass ratio of summation.
7. according to the method described in claim 1, it is characterized by: the reaction time is 1~4h in step b or e.
8. according to the method described in claim 1, it is characterized by: the organic solvent solution mass concentration is 75 in step f
~95%.
9. according to the method described in claim 1, it is characterized by: the organic solvent be ethyl alcohol, isopropanol, the tert-butyl alcohol or
At least one of acetone.
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| CN109503723B (en) * | 2018-11-29 | 2023-04-28 | 瑞红锂电池材料(苏州)有限公司 | Preparation method of nano CMCLi |
| CN111363049A (en) * | 2019-11-21 | 2020-07-03 | 重庆纤磊新材料科技有限公司 | Method for synthesizing ultrahigh-viscosity lithium carboxymethyl cellulose with ultralow solvent system |
| CN111533815A (en) * | 2020-05-14 | 2020-08-14 | 重庆硕盈峰新能源科技有限公司 | Preparation method of nano-crystalline lithium cellulose for lithium battery |
| CN112679619A (en) * | 2020-12-28 | 2021-04-20 | 常熟威怡科技有限公司 | Manufacturing method of sodium carboxymethylcellulose with novel structure |
| CN112724266A (en) * | 2020-12-28 | 2021-04-30 | 常熟威怡科技有限公司 | Preparation method of lithium carboxymethyl cellulose for lithium battery |
| CN115215945A (en) * | 2022-08-08 | 2022-10-21 | 大连中比动力电池有限公司 | Lithium carboxymethyl cellulose and preparation method thereof |
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| CN102206286A (en) * | 2011-05-16 | 2011-10-05 | 北京理工大学 | Preparation method of lithium carboxymethyl cellulose for lithium battery |
| CN105330751A (en) * | 2015-11-05 | 2016-02-17 | 重庆力宏精细化工有限公司 | Continuous production method of carboxymethylcellulose lithium for lithium batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102206286A (en) * | 2011-05-16 | 2011-10-05 | 北京理工大学 | Preparation method of lithium carboxymethyl cellulose for lithium battery |
| CN105330751A (en) * | 2015-11-05 | 2016-02-17 | 重庆力宏精细化工有限公司 | Continuous production method of carboxymethylcellulose lithium for lithium batteries |
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